CN104089858A - Particle size analyzer - Google Patents
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- CN104089858A CN104089858A CN201410346734.5A CN201410346734A CN104089858A CN 104089858 A CN104089858 A CN 104089858A CN 201410346734 A CN201410346734 A CN 201410346734A CN 104089858 A CN104089858 A CN 104089858A
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Abstract
The invention discloses a particle size analyzer which is characterized in that a microscope objective is arranged below an area array sensor; a sample tank is arranged on the focusing plane of the microscope objective; two light sources, namely a transmission light source and a scattering light source are arranged below the sample tank; when micron-grade particles are measured, the transmission light source emits illumination light to illuminate particle samples to be detected, particle images are amplified by the microscope objective to be imaged on an image plane, and image signals obtained after receiving of the images by the area array sensor are transmitted to a computer to be processed to obtain particle size distribution; when nano particles are measured, the transmission light source is turned off while the scattering light source is turned on, laser emitted by the transmission light source is irradiated to nano particle samples, dynamic light scattering signals generated by Brownian movement of the nano particles are received by the area array sensor through the microscope objective, and the obtained signals are transmitted to the computer to be processed to obtain the particle size distribution. According to the particle size analyzer, the particles with the size range from nanometers to hundreds of microns can be measured by only one image sensor, so as to meet the requirements of wide-range particle measurement.
Description
Technical field
The present invention relates to a kind of grain graininess instrument, particularly a kind ofly based on image and dynamic light scattering measurement principle, combine and realize the measurement mechanism from nanometer to micron particles granulometry.
Background technology
Particle sizing method is different according to the granule size of tested particle, has multiple Principle and method of measurement.For the particle of micron order size (from about 1 micron to hundreds of microns), main method is the laser particle analyzer based on light scattering theory, is the static scattered light of measuring particle in laser particle analyzer.Its ultimate principle is when laser incides tested particle; particle meeting scattering incident laser; the space distribution of its scattering luminous energy is relevant with the size of particle, measures the space distribution of its scattering luminous energy, then applies the size-grade distribution that light scattering theory and inversion algorithm can obtain tested particle.In this measuring method and the laser particle analyzer based on the method development, because only consider the scattered light intensity of particle and the relation of grain size, so be called static light scattering method, measure.This method is applicable to submicron particles to the granulometry of micron particles, is subject to the restriction of static light scattering principle, can not measure the granularity of nano particle.For the measurement lower limit of lowering apparatus, some instruments adopts rearward measurement before multi-angle, utilizes the different characteristic of scattered light intensity in different angles of particle to record the granularity of micron particles.
With the development of image sensing device CCD and CMOS, the particle-size measuring instrument device based on image method measuring principle also gets rapid development in recent years.This quasi-instrument is the image of directly measuring each particle, calculates and add up the granularity of each tested particle, obtains size-grade distribution and the mean grain size of tested particle.The feature of image method particle size measuring instrument is that the granularity of each particle is measured, and the size-grade distribution accuracy of acquisition is higher, and it is relevant with the sensing area size of image sensing device with the enlargement ratio of camera lens that it measures the upper limit.But be subject to the restriction of optical principle, image method grain graininess Limit of measurement of apparatus is in general 1 micron of left and right, and the particle sizing error that is less than this lower limit will significantly increase, and maybe cannot measure.
The granulometry of nano particle mainly contains electron microscope and multiple dynamic light scattering nano particle size measuring method theoretical based on dynamic light scattering and development, photon correlation spectroscopy most importantly wherein, Photon correlation spectroscopy, is called for short PCS.
The ultimate principle of PCS nano particles measuring method is to incide tested nano particle when beam of laser
During sample, due to the Brownian movement of nano particle in liquid, its scattered light can be pulsed, and the height of its ripple frequency is relevant with the coefficient of diffusion of particle, and coefficient of diffusion
d t relevant with the granule size of particle, the diffusion of particle and the relation of granularity can be described with Stocks-Einstein formula:
（1）
In formula
k b the graceful constant of bohr thatch,
tabsolute temperature,
ηviscosity,
rit is the radius of particle to be measured.
Classical PCS nano particles method based on above-mentioned theory is measured its scattered light burst length sequence in incident light 90 degree directions with photomultiplier or avalanche diode, adopts correlator deal with data, obtains the coefficient of diffusion of particle
d t , then according to above-mentioned theory, obtain the size-grade distribution of nano particle.This kind of measuring method is existing historical for many years, is the main method that current nano particle is measured, but still comes with some shortcomings, as being obtains enough particle informations, the sampling time requires very long, and apparatus structure is complicated, require tested granule density extremely low, cause sample preparation difficulty etc.
Patent WO2010/149887 has improved this measuring method, adopts the rear orientation light of backward 180 degree angular measurement nano particles, and uses optical fiber incident instead and receive and measure light, can measure the nano particle of high concentration.
Because the scattered light intensity of nano particle is very weak, for obtaining the signal of sufficient intensity, must adopt the laser instrument of relatively high power.Japan Shimadzu company has proposed a kind of new nano particle measuring method and instrument IG-1000 Particle Size Analyzer.In this method, light-sensitive detector part is not the scattered light of measuring nano particle, but the electric field first producing with comb electrode forms grating by tested nano particle, and beam of laser is incided to this grating, measures its diffraction light.Then remove electric field, particle can spread, and now measures the change procedure of diffraction light again, will after Measurement and Data Processing, obtain the size-grade distribution of particle.
Patent GB2318889(NanoSight) a kind of method of measuring each nano particles according to nano particle Brownian movement track following has been proposed.In the method, one hemibase of sample cell plates metal level as thin as a wafer, second half bottom surface, transparent sample pond is plated film not, converge laser beam inciding from the side between sample cell plated film district and border that plated film does not go from sample cell, tested particle is produced compared with strong scattering light by diffraction effect and plasma resonant vibration effect meeting under Ear Mucosa Treated by He Ne Laser Irradiation, at incident light an angle of 90 degrees, with microcobjective, is received.Because particle is done Brownian movement, the scattered light meeting random drift producing when particle is done Brownian movement under Ear Mucosa Treated by He Ne Laser Irradiation, use the random drift movement locus that records each particle with the digital micro-analysis object lens of CCD camera, be the Brownian movement track of tested nano particle, just can obtain according to Stocks-Einstein formula (1) granularity of each particle.
The measurement range of above-mentioned these surveying instruments all can not cover the requirement that measurement range from nanometer to micron meets particle sizing.
Summary of the invention
The object of the invention is in order to overcome the shortcoming of prior art, provide a kind of measurement range to cover nanometer to the grain graininess instrument of the grain graininess of micron.
Ultimate principle of the present invention is that image method measurement and dynamic light scattering method measurement are combined, image and the dynamic light scattering signal of with 1 imageing sensor (CCD, CMOS or other array image sensors), measuring tested particle obtain granularity and the distribution of particle after image and data processing.
When nano particle suspends in liquid, be subject to the unordered shock of a large amount of fluid molecules of periphery, can produce random motion, this motion of particle is called Brownian movement.The ultimate principle of PCS nano particles measuring method is when beam of laser incides tested nano particle sample, due to the Brownian movement of nano particle in liquid, its scattered light can be pulsed, and the height of its ripple frequency is relevant with the coefficient of diffusion of particle, and coefficient of diffusion
d t relevant with the granule size of particle, the diffusion of particle and the relation of granularity can be described with Stocks-Einstein formula:
（1）
In formula
k b the graceful constant of bohr thatch,
tabsolute temperature,
ηviscosity,
rit is the radius of particle to be measured.
Coefficient of diffusion
d t can use the autocorrelation function of scattered light Strong fluctuation and change
g (τ)describe:
（2）
Wherein
i (t),
i (t+ τ)be
tand
t+ τthe particle scattered light light intensity signal constantly recording,
τit is time delay.For monodisperse particles, autocorrelation function is decaying exponential function, can be expressed as:
（3）
In formula:
（4）
（5）
Гwith
qbe called decay live width and scattering wave vector,
nfor the refractive index of dispersion medium,
λ 0 for incident
Optical wavelength,
θfor scattering angle.Thus, the time series signal that records dynamic light scattering carries out autocorrelation calculation and obtains after the autocorrelation function of scattered light fluctuation, just can be by formula (3), and formula (4), formula (5) and formula (1) obtain the granularity of nano particle
d.
For the particle that is greater than several microns, there is not Brownian movement, also just can not measure its granularity by dynamic light scattering method.The measurement lower limit of image method is just in time about 1 micron of left and right, and the upper limit can arrive hundreds of microns.The measurement range of these 2 kinds of methods is complementary, can meet grain graininess and measure the four corner from nanometer to micron.
Based on above-mentioned two kinds of measuring principles, technical scheme of the present invention is: the grain graininess measurement mechanism that a kind of image method and dynamic light scattering combine, it is characterized in that, this measurement mechanism adopts array image sensor as measuring sensor, under described array image sensor, be equipped with microcobjective, on the focal plane of described microcobjective, be equipped with sample cell, under sample cell, be equipped with two light sources, one of them is the transmitted light source that adopts LED or pea lamp, described transmitted light source is arranged on the axis direction of sample cell and microcobjective, another is to adopt the scattering light source of laser instrument to incide on sample cell with the θ angle of 5-90 degree, when measuring the above particle of micron order, the transmitted light source being positioned under sample cell sends illumination light, illuminate the tested particulate samples in sample cell, particle image is being looked like in plane by microcobjective amplification imaging, the picture signal that enlarged image obtains after being received by array image sensor is delivered to computing machine and is carried out image processing, obtains particle size distribution and form factor parameter, when measuring nano particle, close transmitted light source, open scattering light source, the Ear Mucosa Treated by He Ne Laser Irradiation that scattering light source sends is to tested nano particle sample, nano particle is received by array image sensor by microcobjective because of the dynamic light scattering signal that Brownian movement produces, the signal obtaining is delivered to computing machine and is carried out data processing, obtains particle size distribution and form factor parameter.
Described sample cell is cuvette or wave carrier piece.
Described transmitted light source is arranged in the optical axis of sample cell and microcobjective and becomes an angle of 90 degrees, and the light place of intersecting vertically sending at optical axis and the transmitted light source of microcobjective is equipped be all-trans prism or catoptron.By be all-trans prism or catoptron etc., light folding is turn 90 degrees, illuminate the particulate samples on sample cell or microslide.
Described array image sensor is CCD or cmos device.
Described scattering light source laser instrument used is semiconductor laser LD or fiber laser.
Described transmitted light source adopts LED, pea lamp or from optical fiber, scioptics converge, and incides sample cell or microslide, illuminates tested particulate samples.
The invention has the beneficial effects as follows and utilize an imageing sensor, as CCD or CMOS face battle array digital camera
Can measure the particle of particle size range from nanometer to hundreds of microns, meet the requirement of wide region particle sizing, and can form the minitype particle particle size analyzer with wide granulometry scope being easy to carry about with one.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 schematic diagram;
Fig. 2 the present invention is embodiment 2 schematic diagram.
Embodiment
Embodiment 1: the grain graininess measurement mechanism that a kind of image method and dynamic light scattering combine, it is characterized in that, this measurement mechanism adopts array image sensor 1 as measuring sensor, at 1 time layout microcobjective 2 of described array image sensor, on the focal plane of described microcobjective 2, be equipped with sample cell 3, sample cell is equipped with two light sources for 3 times, one of them is the transmitted light source 4 that adopts LED or pea lamp, described transmitted light source 4 is arranged on the axis direction of sample cell 3 and microcobjective 2, another is to adopt the scattering light source 5 of laser instrument to incide on sample cell 3 with the θ angle of 5-90 degree, when measuring the above particle of micron order, the transmitted light source 4 being positioned under sample cell 3 sends illumination light, illuminate the tested particulate samples 6 in sample cell 3, particle image is being looked like in plane by microcobjective 2 amplification imagings, the picture signal that enlarged image obtains after being received by array image sensor 1 is delivered to computing machine and is carried out image processing, obtain particle size distribution and form factor parameter, at this moment scattering light source 5 is not luminous, when measuring nano particle, close transmitted light source 4, open scattering light source 5, the Ear Mucosa Treated by He Ne Laser Irradiation that scattering light source 5 sends is to tested nano particle sample 6, nano particle is received by array image sensor 1 by microcobjective because of the dynamic light scattering signal that Brownian movement produces, the signal obtaining is delivered to computing machine and is carried out data processing, obtains particle size distribution and form factor parameter.
Because the depth of field of microcobjective is very little, for obtaining image clearly, sample cell is arranged on microspur adjusting pole 7, can adjust this support and obtain image clearly during measurement.. when image is processed, if the image obtaining is carried out to pre-service, by the not fuzzy particle image rejecting on focal plane, only process picture rich in detail, this microspur adjusting pole 7 can be cancelled.
While measuring nano particle, the luminous nano particle sample 6 illuminating on sample cell 3 of scattering light source 5, nano particle scatter incident light, the dynamic scattering light of generation is collected through microcobjective, after by imageing sensor 1, detected,
The dynamic light scattering signal obtaining is delivered to computing machine and is carried out data processing, obtains particle size distribution.
Embodiment 2:
Consider when structure needs, make transmitted light source 4 be arranged in sample cell 3 to become with the optical axis of microcobjective 2
An angle of 90 degrees, the light place of intersecting vertically sending at optical axis and the transmitted light source 4 of microcobjective 2 is equipped be all-trans prism or catoptron 8.By be all-trans prism or catoptron 8, light folding is turn 90 degrees, illuminate the particulate samples on sample cell.Particle image is by microcobjective 2 amplification imagings in picture plane, and the picture signal that enlarged image obtains after being received by imageing sensor 1 is delivered to computing machine and carried out image processing, obtains particle size distribution.
Sample cell 3 in embodiment can adopt cuvette or wave carrier piece.Array image sensor 1 in embodiment can adopt CCD or cmos device.Scattering light source 5 laser instrument used is semiconductor laser LD or fiber laser.Transmitted light source 4 adopts LED, pea lamp or from optical fiber, scioptics converge, and incides sample cell or microslide, illuminates tested particulate samples.
Claims (5)
1. a grain graininess instrument, it is characterized in that, this instrument adopts array image sensor (1) as measuring sensor, under described array image sensor, arrange microcobjective (2), on the focal plane of described microcobjective (2), be equipped with sample cell (3), under sample cell (3), be equipped with two light sources, one of them is the transmitted light source (4) that adopts LED or pea lamp, described transmitted light source (4) is arranged on the axis direction of sample cell (3) and microcobjective (2), another is to adopt the scattering light source (5) of laser instrument to incide on sample cell (3) with the θ angle of 5-90 degree, when measuring the above particle of micron order, the transmitted light source (4) being positioned under sample cell (3) sends illumination light, illuminate the tested particulate samples (6) in sample cell (3), particle image is being looked like in plane by microcobjective (2) amplification imaging, the picture signal that enlarged image obtains after being received by array image sensor (1) is delivered to computing machine and is carried out image processing, obtains particle size distribution and form factor parameter, when measuring nano particle, close transmitted light source (4), open scattering light source (5), the Ear Mucosa Treated by He Ne Laser Irradiation that scattering light source (5) sends is to tested nano particle sample (6), nano particle is received by array image sensor (1) by microcobjective because of the dynamic light scattering signal that Brownian movement produces, the signal obtaining is delivered to computing machine and is carried out data processing, obtains particle size distribution and form factor parameter.
2. grain graininess instrument according to claim 1, is characterized in that, described sample cell (3) is cuvette or wave carrier piece.
3. grain graininess instrument according to claim 1, it is characterized in that, described transmitted light source (4) is arranged in sample cell (3) and becomes an angle of 90 degrees with the optical axis of microcobjective (2), and the light place of intersecting vertically sending at optical axis and the transmitted light source (4) of microcobjective (2) is equipped be all-trans prism or catoptron (8).
4. grain graininess instrument according to claim 1, is characterized in that, described array image sensor (1) is CCD or cmos device.
5. grain graininess instrument according to claim 1, is characterized in that, described scattering light source (5) laser instrument used is semiconductor laser LD or fiber laser.
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Cited By (19)
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| CN104568683A (en) * | 2014-12-25 | 2015-04-29 | 上海理工大学 | Nano-particle size measurement device and method |
| CN105043948A (en) * | 2015-08-26 | 2015-11-11 | 清华大学 | Measurement system and method for grain diameter of single nano particle |
| CN105115866A (en) * | 2015-08-26 | 2015-12-02 | 清华大学 | Measurement system and measurement method for particle size of single nano particle |
| CN106066294A (en) * | 2015-04-22 | 2016-11-02 | 罗伯特·博世有限公司 | Particle sensor equipment |
| CN106248532A (en) * | 2016-07-22 | 2016-12-21 | 浙江大学 | The optical detecting method of particle shape and system |
| CN107238558A (en) * | 2017-06-23 | 2017-10-10 | 南京工业大学 | Multifunctional particulate matter sampling device based on CCD/CMOS chip |
| WO2018108646A1 (en) | 2016-12-16 | 2018-06-21 | Koninklijke Philips N.V. | Fanless airborne pollutant sensing |
| EP3382367A1 (en) | 2017-03-30 | 2018-10-03 | Koninklijke Philips N.V. | Fanless airborne pollutant sensing |
| WO2018202909A1 (en) | 2017-05-05 | 2018-11-08 | Koninklijke Philips N.V. | Particulate matter sensing |
| WO2018229171A1 (en) | 2017-06-16 | 2018-12-20 | Koninklijke Philips N.V. | Air pollutant sensing |
| CN109060619A (en) * | 2018-08-24 | 2018-12-21 | 哈尔滨北极星科技有限公司 | A kind of low deuterium-oxide detection device and detection method |
| EP3418720A1 (en) | 2017-06-20 | 2018-12-26 | Koninklijke Philips N.V. | Particulate matter sensing |
| EP3428639A1 (en) | 2017-07-13 | 2019-01-16 | Koninklijke Philips N.V. | Air pollutant sensing |
| CN110044782A (en) * | 2019-05-20 | 2019-07-23 | 西南石油大学 | Across the scale wide spectrum partial size plugging formula Analytical Methods of Grain Grade of one kind |
| CN110286069A (en) * | 2019-07-26 | 2019-09-27 | 佛山科学技术学院 | A kind of Atmospheric particulates scattering observation device |
| CN110879194A (en) * | 2019-12-16 | 2020-03-13 | 深圳市龙岗大工业区混凝土有限公司 | Fineness detection device of concrete aggregate |
| CN111650100A (en) * | 2020-06-16 | 2020-09-11 | 辽东学院 | Particle size measuring equipment based on Mie's scattering theory |
| CN113424041A (en) * | 2019-02-12 | 2021-09-21 | 克里斯多佛·朗哈默 | System and method for detecting the presence of particles in a fluid |
| CN113597546A (en) * | 2019-03-23 | 2021-11-02 | 堀场仪器株式会社 | Improved method for determining nanoparticle size in colloids |
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| CN104568683A (en) * | 2014-12-25 | 2015-04-29 | 上海理工大学 | Nano-particle size measurement device and method |
| CN104568683B (en) * | 2014-12-25 | 2017-08-25 | 上海理工大学 | A kind of nano particles measurement apparatus and method |
| CN106066294A (en) * | 2015-04-22 | 2016-11-02 | 罗伯特·博世有限公司 | Particle sensor equipment |
| CN105043948B (en) * | 2015-08-26 | 2017-09-22 | 清华大学 | The measuring system and measuring method of single nanoparticle particle diameter |
| CN105115866A (en) * | 2015-08-26 | 2015-12-02 | 清华大学 | Measurement system and measurement method for particle size of single nano particle |
| CN105043948A (en) * | 2015-08-26 | 2015-11-11 | 清华大学 | Measurement system and method for grain diameter of single nano particle |
| CN106248532A (en) * | 2016-07-22 | 2016-12-21 | 浙江大学 | The optical detecting method of particle shape and system |
| WO2018108646A1 (en) | 2016-12-16 | 2018-06-21 | Koninklijke Philips N.V. | Fanless airborne pollutant sensing |
| EP3382367A1 (en) | 2017-03-30 | 2018-10-03 | Koninklijke Philips N.V. | Fanless airborne pollutant sensing |
| WO2018202909A1 (en) | 2017-05-05 | 2018-11-08 | Koninklijke Philips N.V. | Particulate matter sensing |
| WO2018229171A1 (en) | 2017-06-16 | 2018-12-20 | Koninklijke Philips N.V. | Air pollutant sensing |
| EP3418720A1 (en) | 2017-06-20 | 2018-12-26 | Koninklijke Philips N.V. | Particulate matter sensing |
| CN107238558A (en) * | 2017-06-23 | 2017-10-10 | 南京工业大学 | Multifunctional particulate matter sampling device based on CCD/CMOS chip |
| EP3428639A1 (en) | 2017-07-13 | 2019-01-16 | Koninklijke Philips N.V. | Air pollutant sensing |
| CN109060619A (en) * | 2018-08-24 | 2018-12-21 | 哈尔滨北极星科技有限公司 | A kind of low deuterium-oxide detection device and detection method |
| CN109060619B (en) * | 2018-08-24 | 2024-02-23 | 哈尔滨北极星科技有限公司 | Deuterium-depleted water detection device and detection method |
| CN113424041A (en) * | 2019-02-12 | 2021-09-21 | 克里斯多佛·朗哈默 | System and method for detecting the presence of particles in a fluid |
| CN113597546A (en) * | 2019-03-23 | 2021-11-02 | 堀场仪器株式会社 | Improved method for determining nanoparticle size in colloids |
| CN113597546B (en) * | 2019-03-23 | 2022-10-28 | 堀场仪器株式会社 | Improved method for determining nanoparticle size in colloids |
| CN115655986B (en) * | 2019-03-23 | 2023-06-27 | 堀场仪器株式会社 | Improved method for determining the size of nanoparticles in colloids |
| CN110044782A (en) * | 2019-05-20 | 2019-07-23 | 西南石油大学 | Across the scale wide spectrum partial size plugging formula Analytical Methods of Grain Grade of one kind |
| CN110044782B (en) * | 2019-05-20 | 2019-10-11 | 西南石油大学 | Across the scale wide spectrum partial size plugging formula Analytical Methods of Grain Grade of one kind |
| US10782220B1 (en) | 2019-05-20 | 2020-09-22 | Southwest Petroleum University | Cross-scale wide-spectrum particle size plugging formula granularity analysis method |
| CN110286069A (en) * | 2019-07-26 | 2019-09-27 | 佛山科学技术学院 | A kind of Atmospheric particulates scattering observation device |
| CN110879194A (en) * | 2019-12-16 | 2020-03-13 | 深圳市龙岗大工业区混凝土有限公司 | Fineness detection device of concrete aggregate |
| CN110879194B (en) * | 2019-12-16 | 2022-08-23 | 深圳市龙岗大工业区混凝土有限公司 | Fineness detection device of concrete aggregate |
| CN111650100A (en) * | 2020-06-16 | 2020-09-11 | 辽东学院 | Particle size measuring equipment based on Mie's scattering theory |
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Application publication date: 20141008 |